Sample loss

Frequently, preconcentration of an analyte is necessary because the detector used for quantitation may not have the necessary detectabiUty, selectivity, or freedom from matrix interferences (32). Significant sample losses can occur during this step because of very small volume losses to glass walls of the recovery containers, pipets, and other glassware. 

Can work with two LC modes that Sample loss or contamination... 

For the storage of a substance dissolved in a volatile solvent, the solution must be placed directly in the flask, not within a vial. During the evacuation, gently sway the flask and adjust the evacuation speed to avoid sample loss due to a sudden boiling of the solution. Replace the inside space of the flask completely with the solvent vapor (typically methanol) by boiling the sample solution for a period of 1-2 minutes before closing the stopcock. In using this method, however,... 

It is possible to carry out a chromatographic separation, collect all, or selected, fractions and then, after removal of the majority of the volatile solvent, transfer the analyte to the mass spectrometer by using the conventional inlet (probe) for solid analytes. The direct coupling of the two techniques is advantageous in many respects, including the speed of analysis, the convenience, particularly for the analysis of multi-component mixtures, the reduced possibility of sample loss, the ability to carry out accurate quantitation using isotopically labelled internal standards, and the ability to carry out certain tasks, such as the evaluation of peak purity, which would not otherwise be possible. 

One approach to the problem of matrix effects is to prevent the matrix materials reaching the electrospray source by carrying out some form of clean-up prior to analysis and/or to employ chromatographic separation. It is not always possible, however, to develop a simple procedure for sample clean-up and since this approach involves further work-up with the associated increase in analysis time and potential for sample loss it is therefore not ideal. 

Another significant difference between large- and small-scale processing is dilution of the product samples with water. Food processing equipment for fluids often needs to be started with water, and the food needs to be flushed from the system with water before the process is shut down. When making small batch samples in this type of equipment, care must be taken to obtain a representative sample with a minimum of dilution. There will also be a difference in the weights of the sample into and out of the process due to water addition or sample loss to minimize dilution. 

LC/MS/MS is used to measure the ratio of analyte to internal standard in the sample and standard (the relative response determination). Once the internal standard has been added to the sample extract or standard solution, the analyte/IS ratio will not change. Subsequent sample losses will not change the analyte/IS ratio, nor will sample dilutions, solvent evaporation, changes in instrumental response or loss of chromatographic resolution. 

Freeze Conceit tret ion Hater sample is partially frozen, concentrating the dissolved substances in the unfrozen portion. All sample types Minimizes sample losses due to volatilization or chemical modification. Principal losses occur due to occlusion, adsorption, evaporation and channelling in the ice layer. Limited sample size. 

Many of the classical techniques used in the preparation of samples for chromatography are labour-intensive, cumbersome, and prone to sample loss caused by multistep manual manipulations. During the past few years, miniaturisation has become a dominant trend in analytical chemistry. At the same time, work in GC and UPLC has focused on improved injection techniques and on increasing speed, sensitivity and efficiency. Separation times for both techniques are now measured in minutes. Miniaturised sample preparation techniques in combination with state-of-the-art analytical instrumentation result in faster analysis, higher sample throughput, lower solvent consumption, less manpower in sample preparation, while maintaining or even improving limits. 

Where aqueous NMS solutions are used as the feedstock, higher NMP 2P product ratios are generally observed. However, when aqueous NMS feed is run at 265°C, free methanol is observed in the earliest product samples. Loss of the methyl group from NMS via high temperature hydrolysis apparently becomes significant at this temperature. With aqueous NMS as the feedstock, and when the reaction temperature is lowered to 200°C, NMP 2P molar product ratios as high 67 1 were observed for the more active 2.5%Rh2.5%Re/C catalyst. At the same temperature, even the less active 2.5%Rh2.5%Zr/C catalyst displayed a respectable NMP 2P product ratio of 38 1. 

However, pyrolysis is rapid, avoids sample wet chemical workup, avoiding sample loss and contamination, and has a low sample requirement. It allows the determination, in a single step, of polymeric materials (with in situ hydrolysis of the hydrolysable polymers and thermal decomposition of the nonhydrolysable polymers) and low molecular weight components [16]. As a result, pyrolysis is a relatively fast and inexpensive technique, especially if compared with the classical wet analytical procedures that are required prior to GC/MS analyses. 

During the storage of the sample, loss of analyte can occur via vaporisation, degradation, and/or adsorption. Adsorption of trace organic and inorganic species in seawater to container walls can severely affect the accuracy of their determination. The adsorption of dichlorodiphenyltrichloroethylene [67] and hexachlorobiphenyl [68] onto glass containers has been observed. 

In the case of static sampling, the material of the bag should have the same properties as given before and, moreover, should suffer no sample losses by diffusion. Good experiences have so far been made with PFTE, TEDLAR and Polyamid bags. 

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